# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Andreas Schnepf' _publ_contact_author_email SCHNEPF@CHEMIE.UNI-KARLSRUHE.DE _publ_section_title ; [(OtBu)2C6H3]3Ge+ a Free Germyl Cation with Aryl Ligands ; loop_ _publ_author_name 'Andreas Schnepf' 'Christian Drost' 'Christian Schenk' # Attachment 'AS112mon.cif' data_as112mon _database_code_depnum_ccdc_archive 'CCDC 698439' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C59.88 H66.75 Al Cl3.75 F36 Ge O10' _chemical_formula_weight 1862.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 18.1010(9) _cell_length_b 24.3749(8) _cell_length_c 18.2722(8) _cell_angle_alpha 90.00 _cell_angle_beta 106.088(4) _cell_angle_gamma 90.00 _cell_volume 7746.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 99(2) _cell_measurement_reflns_used 69390 _cell_measurement_theta_min 1.40 _cell_measurement_theta_max 25.795 _exptl_crystal_description fragment _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.597 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3755 _exptl_absorpt_coefficient_mu 0.674 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7708 _exptl_absorpt_correction_T_max 0.8189 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 99(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54448 _diffrn_reflns_av_R_equivalents 0.0614 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 26.06 _reflns_number_total 15111 _reflns_number_gt 12332 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+6.5783P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15111 _refine_ls_number_parameters 1136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0569 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1138 _refine_ls_wR_factor_gt 0.1068 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ge1 Ge 0.248106(13) 0.505049(10) 0.241995(14) 0.02595(7) Uani 1 1 d . . . Al1 Al 0.27237(4) 0.24827(3) 0.82398(4) 0.02627(15) Uani 1 1 d . . . O1 O 0.24521(10) 0.19892(7) 0.75384(10) 0.0326(4) Uani 1 1 d . . . O2 O 0.22749(10) 0.24058(7) 0.89541(10) 0.0327(4) Uani 1 1 d . . . O3 O 0.37012(9) 0.24139(7) 0.86407(10) 0.0323(4) Uani 1 1 d . . . O4 O 0.24748(10) 0.31156(7) 0.78196(10) 0.0336(4) Uani 1 1 d . A . O5 O 0.36758(10) 0.58491(8) 0.29228(10) 0.0399(4) Uani 1 1 d . . . O6 O 0.20754(10) 0.50767(7) 0.07808(10) 0.0328(4) Uani 1 1 d . . . O16 O 0.26081(11) 0.49678(8) 0.40243(10) 0.0385(4) Uani 1 1 d . . . O17 O 0.34841(10) 0.42209(8) 0.21201(11) 0.0406(4) Uani 1 1 d . . . O26 O 0.13982(9) 0.41614(7) 0.20216(10) 0.0317(4) Uani 1 1 d . . . O27 O 0.16056(10) 0.59856(7) 0.26686(11) 0.0356(4) Uani 1 1 d . . . C1 C 0.29163(13) 0.54995(10) 0.17987(14) 0.0292(5) Uani 1 1 d . . . C2 C 0.26310(13) 0.54707(10) 0.10069(14) 0.0304(5) Uani 1 1 d . . . C3 C 0.29507(15) 0.57970(11) 0.05543(15) 0.0377(6) Uani 1 1 d . . . H3 H 0.2760 0.5787 0.0015 0.045 Uiso 1 1 calc R . . C4 C 0.35594(16) 0.61408(12) 0.09106(17) 0.0421(6) Uani 1 1 d . . . H4 H 0.3783 0.6364 0.0603 0.051 Uiso 1 1 calc R . . C5 C 0.38519(16) 0.61707(12) 0.16962(17) 0.0417(6) Uani 1 1 d . . . H5 H 0.4270 0.6407 0.1922 0.050 Uiso 1 1 calc R . . C6 C 0.35219(14) 0.58496(11) 0.21443(15) 0.0338(5) Uani 1 1 d . . . C8C C 0.4308(2) 0.58032(15) 0.42059(18) 0.0608(9) Uani 1 1 d . . . H8C1 H 0.3882 0.6013 0.4300 0.091 Uiso 1 1 calc R . . H8C2 H 0.4778 0.5873 0.4616 0.091 Uiso 1 1 calc R . . H8C3 H 0.4186 0.5411 0.4190 0.091 Uiso 1 1 calc R . . C8 C 0.44304(16) 0.59767(13) 0.34519(17) 0.0453(7) Uani 1 1 d . . . C8B C 0.5046(2) 0.56383(18) 0.3256(2) 0.0706(11) Uani 1 1 d . . . H8B1 H 0.4922 0.5248 0.3273 0.106 Uiso 1 1 calc R . . H8B2 H 0.5543 0.5713 0.3625 0.106 Uiso 1 1 calc R . . H8B3 H 0.5073 0.5734 0.2743 0.106 Uiso 1 1 calc R . . C8A C 0.4584(2) 0.65892(14) 0.3460(2) 0.0601(9) Uani 1 1 d . . . H8A1 H 0.4731 0.6691 0.3001 0.090 Uiso 1 1 calc R . . H8A2 H 0.5002 0.6683 0.3912 0.090 Uiso 1 1 calc R . . H8A3 H 0.4118 0.6789 0.3472 0.090 Uiso 1 1 calc R . . C9C C 0.09715(16) 0.46126(12) 0.01238(16) 0.0403(6) Uani 1 1 d . . . H9C1 H 0.1251 0.4272 0.0303 0.061 Uiso 1 1 calc R . . H9C2 H 0.0585 0.4546 -0.0363 0.061 Uiso 1 1 calc R . . H9C3 H 0.0716 0.4740 0.0501 0.061 Uiso 1 1 calc R . . C9B C 0.11214(15) 0.55930(11) -0.01888(15) 0.0377(6) Uani 1 1 d . . . H9B1 H 0.0903 0.5707 0.0222 0.057 Uiso 1 1 calc R . . H9B2 H 0.0708 0.5553 -0.0663 0.057 Uiso 1 1 calc R . . H9B3 H 0.1488 0.5871 -0.0258 0.057 Uiso 1 1 calc R . . C9A C 0.19325(16) 0.48514(12) -0.05658(15) 0.0380(6) Uani 1 1 d . . . H9A1 H 0.2278 0.5139 -0.0651 0.057 Uiso 1 1 calc R . . H9A2 H 0.1547 0.4768 -0.1047 0.057 Uiso 1 1 calc R . . H9A3 H 0.2231 0.4520 -0.0375 0.057 Uiso 1 1 calc R . . C9 C 0.15330(14) 0.50478(11) 0.00161(14) 0.0328(5) Uani 1 1 d . . . C10 C 0.30963(13) 0.45553(10) 0.31306(14) 0.0291(5) Uani 1 1 d . . . C11 C 0.30481(14) 0.45498(11) 0.38810(15) 0.0331(5) Uani 1 1 d . . . C12 C 0.34531(16) 0.41558(12) 0.43806(16) 0.0411(6) Uani 1 1 d . . . H12 H 0.3413 0.4134 0.4887 0.049 Uiso 1 1 calc R . . C13 C 0.39188(16) 0.37934(12) 0.41247(16) 0.0425(7) Uani 1 1 d . . . H13 H 0.4200 0.3526 0.4469 0.051 Uiso 1 1 calc R . . C14 C 0.39915(15) 0.38039(12) 0.33913(16) 0.0400(6) Uani 1 1 d . . . H14 H 0.4329 0.3558 0.3241 0.048 Uiso 1 1 calc R . . C15 C 0.35605(14) 0.41822(11) 0.28799(15) 0.0335(5) Uani 1 1 d . . . C16C C 0.2990(2) 0.51194(16) 0.54129(18) 0.0572(9) Uani 1 1 d . . . H16A H 0.3320 0.4794 0.5530 0.086 Uiso 1 1 calc R . . H16B H 0.2786 0.5202 0.5845 0.086 Uiso 1 1 calc R . . H16C H 0.3290 0.5433 0.5318 0.086 Uiso 1 1 calc R . . C16 C 0.23231(17) 0.50093(13) 0.47044(15) 0.0422(6) Uani 1 1 d . . . C16B C 0.1864(2) 0.45025(15) 0.4774(2) 0.0565(8) Uani 1 1 d . . . H16D H 0.1447 0.4453 0.4304 0.085 Uiso 1 1 calc R . . H16E H 0.1645 0.4546 0.5205 0.085 Uiso 1 1 calc R . . H16F H 0.2201 0.4181 0.4858 0.085 Uiso 1 1 calc R . . C16A C 0.18088(19) 0.55079(14) 0.45270(17) 0.0504(8) Uani 1 1 d . . . H16G H 0.2106 0.5824 0.4435 0.076 Uiso 1 1 calc R . . H16H H 0.1604 0.5587 0.4959 0.076 Uiso 1 1 calc R . . H16I H 0.1383 0.5437 0.4072 0.076 Uiso 1 1 calc R . . C17A C 0.4049(2) 0.33970(13) 0.17128(19) 0.0547(8) Uani 1 1 d . . . H17A H 0.4270 0.3249 0.2226 0.082 Uiso 1 1 calc R . . H17B H 0.4356 0.3274 0.1378 0.082 Uiso 1 1 calc R . . H17C H 0.3520 0.3266 0.1514 0.082 Uiso 1 1 calc R . . C17 C 0.40521(15) 0.40212(12) 0.17457(16) 0.0393(6) Uani 1 1 d . . . C17C C 0.48403(18) 0.42502(16) 0.2129(2) 0.0572(8) Uani 1 1 d . . . H17D H 0.4816 0.4652 0.2132 0.086 Uiso 1 1 calc R . . H17E H 0.5203 0.4132 0.1850 0.086 Uiso 1 1 calc R . . H17F H 0.5013 0.4115 0.2654 0.086 Uiso 1 1 calc R . . C17B C 0.3736(2) 0.42471(15) 0.09407(18) 0.0532(8) Uani 1 1 d . . . H17G H 0.3204 0.4125 0.0731 0.080 Uiso 1 1 calc R . . H17H H 0.4050 0.4112 0.0619 0.080 Uiso 1 1 calc R . . H17I H 0.3753 0.4649 0.0956 0.080 Uiso 1 1 calc R . . C20 C 0.14129(13) 0.50745(10) 0.23387(13) 0.0272(5) Uani 1 1 d . . . C21 C 0.09902(13) 0.45894(10) 0.22028(13) 0.0280(5) Uani 1 1 d . . . C22 C 0.02296(14) 0.45924(11) 0.22188(14) 0.0327(5) Uani 1 1 d . . . H22 H -0.0065 0.4264 0.2138 0.039 Uiso 1 1 calc R . . C23 C -0.00934(14) 0.50847(12) 0.23549(16) 0.0373(6) Uani 1 1 d . . . H23 H -0.0616 0.5087 0.2364 0.045 Uiso 1 1 calc R . . C24 C 0.03155(15) 0.55743(12) 0.24782(15) 0.0370(6) Uani 1 1 d . . . H24 H 0.0077 0.5906 0.2563 0.044 Uiso 1 1 calc R . . C25 C 0.10850(14) 0.55659(10) 0.24748(14) 0.0306(5) Uani 1 1 d . . . C26 C 0.12357(15) 0.35818(11) 0.21304(16) 0.0359(6) Uani 1 1 d . . . C26C C 0.19369(17) 0.33013(12) 0.2010(2) 0.0495(8) Uani 1 1 d . . . H26A H 0.1999 0.3407 0.1513 0.074 Uiso 1 1 calc R . . H26B H 0.1873 0.2903 0.2027 0.074 Uiso 1 1 calc R . . H26C H 0.2393 0.3412 0.2413 0.074 Uiso 1 1 calc R . . C26B C 0.05227(17) 0.33943(12) 0.15169(19) 0.0484(7) Uani 1 1 d . . . H26D H 0.0062 0.3545 0.1625 0.073 Uiso 1 1 calc R . . H26E H 0.0497 0.2993 0.1513 0.073 Uiso 1 1 calc R . . H26F H 0.0552 0.3525 0.1018 0.073 Uiso 1 1 calc R . . C26A C 0.11750(19) 0.34949(13) 0.29297(19) 0.0519(8) Uani 1 1 d . . . H26G H 0.1637 0.3639 0.3296 0.078 Uiso 1 1 calc R . . H26H H 0.1127 0.3102 0.3020 0.078 Uiso 1 1 calc R . . H26I H 0.0721 0.3688 0.2992 0.078 Uiso 1 1 calc R . . C27 C 0.14028(17) 0.65602(11) 0.24676(17) 0.0407(6) Uani 1 1 d . . . C27C C 0.0965(2) 0.65958(14) 0.16277(19) 0.0545(8) Uani 1 1 d . . . H27A H 0.1255 0.6405 0.1324 0.082 Uiso 1 1 calc R . . H27B H 0.0900 0.6982 0.1473 0.082 Uiso 1 1 calc R . . H27C H 0.0459 0.6424 0.1545 0.082 Uiso 1 1 calc R . . C27B C 0.21857(19) 0.68268(13) 0.2618(2) 0.0562(8) Uani 1 1 d . . . H27D H 0.2478 0.6764 0.3149 0.084 Uiso 1 1 calc R . . H27E H 0.2123 0.7222 0.2523 0.084 Uiso 1 1 calc R . . H27F H 0.2463 0.6667 0.2279 0.084 Uiso 1 1 calc R . . C27A C 0.0975(2) 0.68015(14) 0.3003(2) 0.0628(9) Uani 1 1 d . . . H27G H 0.0447 0.6662 0.2864 0.094 Uiso 1 1 calc R . . H27H H 0.0968 0.7202 0.2961 0.094 Uiso 1 1 calc R . . H27I H 0.1236 0.6695 0.3528 0.094 Uiso 1 1 calc R . . C110 C 0.25412(14) 0.14696(11) 0.73182(14) 0.0324(5) Uani 1 1 d . . . C111 C 0.33505(17) 0.13926(13) 0.71909(18) 0.0451(7) Uani 1 1 d . . . C112 C 0.19151(16) 0.13690(12) 0.65529(16) 0.0398(6) Uani 1 1 d . . . C113 C 0.24343(17) 0.10505(11) 0.79143(17) 0.0417(6) Uani 1 1 d . . . C120 C 0.16424(14) 0.24834(10) 0.91987(15) 0.0333(5) Uani 1 1 d . . . C121 C 0.09507(18) 0.21687(14) 0.8698(2) 0.0557(9) Uani 1 1 d . . . C122 C 0.1829(2) 0.22699(15) 1.0034(2) 0.0567(9) Uani 1 1 d . . . C123 C 0.14392(16) 0.31004(12) 0.92014(19) 0.0447(7) Uani 1 1 d . . . C130 C 0.43093(14) 0.25422(11) 0.92394(15) 0.0338(6) Uani 1 1 d . . . C131 C 0.50482(16) 0.23511(13) 0.90484(18) 0.0434(7) Uani 1 1 d . . . C132 C 0.43531(15) 0.31725(12) 0.93712(16) 0.0399(6) Uani 1 1 d . . . C133 C 0.42454(16) 0.22532(13) 0.99779(17) 0.0444(7) Uani 1 1 d . . . C140 C 0.23735(15) 0.34297(11) 0.71855(15) 0.0339(6) Uani 1 1 d . . . C141 C 0.3128(6) 0.3440(4) 0.6947(6) 0.050(2) Uani 0.558(4) 1 d P A 1 C142 C 0.2193(7) 0.4013(6) 0.7425(10) 0.052(3) Uani 0.558(4) 1 d P A 1 C143 C 0.1686(11) 0.3199(5) 0.6551(10) 0.053(3) Uani 0.558(4) 1 d P A 1 C144 C 0.2943(7) 0.3277(5) 0.6708(6) 0.041(2) Uani 0.442(4) 1 d P A 2 C145 C 0.2502(9) 0.4043(7) 0.7398(10) 0.053(4) Uani 0.442(4) 1 d P A 2 C146 C 0.1563(13) 0.3372(7) 0.6645(14) 0.052(4) Uani 0.442(4) 1 d P A 2 F11C F 0.33810(11) 0.09496(8) 0.67601(11) 0.0597(5) Uani 1 1 d . . . F11B F 0.38874(9) 0.13214(8) 0.78490(11) 0.0549(5) Uani 1 1 d . . . F11A F 0.35503(10) 0.18252(8) 0.68520(11) 0.0559(5) Uani 1 1 d . . . F12C F 0.18221(11) 0.08361(7) 0.63759(10) 0.0541(5) Uani 1 1 d . . . F12B F 0.21057(11) 0.16167(8) 0.59741(9) 0.0517(4) Uani 1 1 d . . . F12A F 0.12428(9) 0.15677(7) 0.65751(9) 0.0462(4) Uani 1 1 d . . . F13C F 0.28037(10) 0.12174(7) 0.86187(9) 0.0487(4) Uani 1 1 d . . . F13B F 0.27033(12) 0.05553(7) 0.78214(11) 0.0579(5) Uani 1 1 d . . . F13A F 0.16933(10) 0.09921(7) 0.78858(10) 0.0491(4) Uani 1 1 d . . . F21C F 0.02768(10) 0.23256(9) 0.87988(14) 0.0667(6) Uani 1 1 d . . . F21B F 0.09040(10) 0.22282(11) 0.79659(12) 0.0722(6) Uani 1 1 d . . . F21A F 0.10251(12) 0.16276(8) 0.88537(17) 0.0800(7) Uani 1 1 d . . . F22C F 0.11885(13) 0.21979(10) 1.02566(14) 0.0774(7) Uani 1 1 d . . . F22B F 0.21864(13) 0.17900(9) 1.01020(13) 0.0715(6) Uani 1 1 d . . . F22A F 0.22825(13) 0.26164(11) 1.05160(11) 0.0736(6) Uani 1 1 d . . . F23C F 0.09695(10) 0.32091(7) 0.96319(11) 0.0533(5) Uani 1 1 d . . . F23B F 0.20677(11) 0.33985(7) 0.94478(14) 0.0641(6) Uani 1 1 d . . . F23A F 0.10836(11) 0.32733(8) 0.84961(12) 0.0616(5) Uani 1 1 d . . . F31C F 0.51246(10) 0.18075(8) 0.91175(11) 0.0540(5) Uani 1 1 d . . . F31B F 0.56861(9) 0.25750(8) 0.95062(12) 0.0581(5) Uani 1 1 d . . . F31A F 0.50302(10) 0.24801(8) 0.83363(11) 0.0516(4) Uani 1 1 d . . . F32C F 0.48403(10) 0.33150(8) 1.00410(10) 0.0525(4) Uani 1 1 d . . . F32B F 0.45904(10) 0.34249(7) 0.88249(10) 0.0485(4) Uani 1 1 d . . . F32A F 0.36675(9) 0.33748(7) 0.93522(10) 0.0450(4) Uani 1 1 d . . . F33C F 0.40005(11) 0.17380(8) 0.98257(10) 0.0543(5) Uani 1 1 d . . . F33B F 0.49120(10) 0.22369(9) 1.05159(10) 0.0615(5) Uani 1 1 d . . . F33A F 0.37409(10) 0.25075(8) 1.02704(9) 0.0501(4) Uani 1 1 d . . . F41A F 0.30079(11) 0.36400(8) 0.62184(11) 0.0581(5) Uani 1 1 d . . . F41B F 0.3652(2) 0.37479(18) 0.7385(2) 0.0651(13) Uani 0.558(4) 1 d P A 1 F41C F 0.3403(4) 0.2929(2) 0.6946(4) 0.0607(14) Uani 0.558(4) 1 d P A 1 F41D F 0.3623(4) 0.3147(3) 0.7158(4) 0.0529(17) Uani 0.442(4) 1 d P A 2 F41E F 0.2666(3) 0.28129(17) 0.6279(2) 0.0558(14) Uani 0.442(4) 1 d P A 2 F42A F 0.22538(13) 0.43831(7) 0.68586(12) 0.0651(5) Uani 1 1 d . . . F42B F 0.1477(2) 0.40521(15) 0.7460(3) 0.0670(13) Uani 0.558(4) 1 d P A 1 F42C F 0.2659(3) 0.41658(19) 0.8084(3) 0.0602(13) Uani 0.558(4) 1 d P A 1 F42D F 0.2190(4) 0.4165(2) 0.7946(4) 0.0604(17) Uani 0.442(4) 1 d P A 2 F42E F 0.3280(3) 0.4128(2) 0.7684(3) 0.0694(17) Uani 0.442(4) 1 d P A 2 F43A F 0.14339(11) 0.35670(9) 0.59796(11) 0.0639(5) Uani 1 1 d . . . F43B F 0.1129(3) 0.3048(3) 0.6833(3) 0.0611(13) Uani 0.558(4) 1 d P A 1 F43C F 0.1910(3) 0.27780(15) 0.62033(18) 0.0623(12) Uani 0.558(4) 1 d P A 1 F43D F 0.1320(4) 0.2845(2) 0.6608(4) 0.0540(15) Uani 0.442(4) 1 d P A 2 F43E F 0.1043(3) 0.3653(2) 0.6944(3) 0.0719(18) Uani 0.442(4) 1 d P A 2 C200 C 0.3053(2) 0.22271(19) 0.4915(3) 0.0780(12) Uani 1 1 d . . . H20A H 0.2951 0.1846 0.4727 0.094 Uiso 1 1 calc R . . H20B H 0.2857 0.2267 0.5366 0.094 Uiso 1 1 calc R . . Cl1 Cl 0.25625(6) 0.26714(5) 0.42152(8) 0.0876(4) Uani 1 1 d . . . Cl2 Cl 0.40466(6) 0.23393(4) 0.51885(6) 0.0700(3) Uani 1 1 d . . . C210 C 0.4680(5) 0.5269(3) 0.9883(5) 0.0619(18) Uani 0.50 1 d P . . H21A H 0.4196 0.5075 0.9870 0.074 Uiso 0.50 1 calc PR . . H21B H 0.4698 0.5500 0.9442 0.074 Uiso 0.50 1 calc PR . . Cl10 Cl 0.4501(4) 0.4734(2) 0.9237(4) 0.114(2) Uani 0.50 1 d P . . Cl11 Cl 0.4471(2) 0.4857(2) 0.9369(3) 0.111(2) Uani 0.50 1 d P . . C220 C 0.0062(7) 0.4488(6) 0.5153(9) 0.101(5) Uani 0.38 1 d P . . H22A H -0.0323 0.4281 0.5336 0.121 Uiso 0.38 1 calc PR . . H22B H 0.0493 0.4235 0.5165 0.121 Uiso 0.38 1 calc PR . . Cl50 Cl 0.0398(3) 0.5007(3) 0.5768(2) 0.1006(16) Uani 0.38 1 d P . . Cl51 Cl 0.0347(3) 0.53252(16) 0.5763(3) 0.0783(11) Uani 0.38 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ge1 0.02220(12) 0.02772(13) 0.02645(13) 0.00268(10) 0.00426(9) -0.00042(10) Al1 0.0251(3) 0.0271(4) 0.0262(4) -0.0028(3) 0.0064(3) -0.0011(3) O1 0.0346(9) 0.0302(9) 0.0315(9) -0.0056(7) 0.0064(7) 0.0014(7) O2 0.0289(9) 0.0383(10) 0.0325(9) -0.0033(8) 0.0113(7) -0.0014(7) O3 0.0269(8) 0.0382(10) 0.0300(9) -0.0040(8) 0.0048(7) -0.0009(7) O4 0.0368(9) 0.0315(9) 0.0316(9) 0.0013(7) 0.0080(7) 0.0011(7) O5 0.0341(9) 0.0513(12) 0.0308(9) -0.0022(9) 0.0032(7) -0.0113(8) O6 0.0356(9) 0.0333(9) 0.0269(8) 0.0026(7) 0.0044(7) -0.0084(7) O16 0.0484(11) 0.0382(10) 0.0283(9) 0.0035(8) 0.0096(8) 0.0094(8) O17 0.0346(10) 0.0503(12) 0.0358(10) -0.0001(9) 0.0083(8) 0.0147(8) O26 0.0297(9) 0.0292(9) 0.0376(10) 0.0002(7) 0.0114(7) -0.0015(7) O27 0.0305(9) 0.0297(9) 0.0420(10) -0.0025(8) 0.0024(7) -0.0006(7) C1 0.0258(11) 0.0306(12) 0.0296(12) -0.0007(10) 0.0049(9) 0.0007(9) C2 0.0277(12) 0.0290(12) 0.0340(13) 0.0018(10) 0.0077(10) -0.0002(10) C3 0.0401(14) 0.0414(15) 0.0310(13) 0.0065(11) 0.0092(11) -0.0053(12) C4 0.0398(15) 0.0467(16) 0.0411(15) 0.0078(13) 0.0131(12) -0.0103(12) C5 0.0356(14) 0.0453(16) 0.0433(16) 0.0003(13) 0.0094(12) -0.0146(12) C6 0.0286(12) 0.0376(14) 0.0339(13) -0.0014(11) 0.0063(10) -0.0039(10) C8C 0.068(2) 0.063(2) 0.0372(16) 0.0005(15) -0.0089(15) -0.0229(17) C8 0.0372(15) 0.0489(17) 0.0413(16) -0.0077(13) -0.0034(12) -0.0111(13) C8B 0.0457(19) 0.079(3) 0.076(3) -0.004(2) -0.0012(17) 0.0090(18) C8A 0.073(2) 0.056(2) 0.0516(19) -0.0182(16) 0.0164(17) -0.0273(17) C9C 0.0399(14) 0.0409(15) 0.0378(14) -0.0013(12) 0.0066(11) -0.0086(12) C9B 0.0364(14) 0.0384(14) 0.0352(14) 0.0003(12) 0.0045(11) 0.0016(11) C9A 0.0437(15) 0.0380(14) 0.0318(13) -0.0012(11) 0.0092(11) 0.0021(12) C9 0.0337(13) 0.0351(13) 0.0266(12) 0.0007(10) 0.0035(10) -0.0035(10) C10 0.0270(11) 0.0286(12) 0.0290(12) 0.0000(10) 0.0034(9) -0.0026(9) C11 0.0328(13) 0.0310(13) 0.0328(13) -0.0002(11) 0.0045(10) -0.0005(10) C12 0.0465(16) 0.0404(15) 0.0308(13) 0.0070(12) 0.0013(11) 0.0046(12) C13 0.0416(15) 0.0366(14) 0.0398(15) 0.0067(12) -0.0046(12) 0.0054(12) C14 0.0327(13) 0.0388(15) 0.0425(15) 0.0015(12) 0.0005(11) 0.0090(11) C15 0.0274(12) 0.0372(14) 0.0324(13) -0.0004(11) 0.0022(10) 0.0008(10) C16C 0.062(2) 0.067(2) 0.0369(16) -0.0084(15) 0.0028(14) 0.0081(17) C16 0.0515(16) 0.0495(17) 0.0261(12) 0.0020(12) 0.0114(11) 0.0067(13) C16B 0.067(2) 0.059(2) 0.0478(18) 0.0048(16) 0.0225(16) 0.0029(17) C16A 0.0615(19) 0.0538(19) 0.0368(15) -0.0007(14) 0.0152(14) 0.0141(15) C17A 0.072(2) 0.0416(17) 0.0487(18) -0.0084(14) 0.0136(16) 0.0066(15) C17 0.0350(14) 0.0399(15) 0.0440(15) -0.0048(12) 0.0126(11) 0.0089(11) C17C 0.0400(16) 0.069(2) 0.064(2) -0.0060(18) 0.0177(15) -0.0034(15) C17B 0.0604(19) 0.059(2) 0.0439(17) 0.0047(15) 0.0207(15) 0.0219(16) C20 0.0261(11) 0.0303(12) 0.0237(11) 0.0030(9) 0.0045(9) 0.0009(9) C21 0.0267(11) 0.0317(12) 0.0238(11) 0.0015(10) 0.0043(9) 0.0005(9) C22 0.0266(12) 0.0384(14) 0.0319(13) -0.0002(11) 0.0064(10) -0.0041(10) C23 0.0240(12) 0.0470(15) 0.0398(14) 0.0003(12) 0.0070(10) 0.0005(11) C24 0.0303(13) 0.0390(14) 0.0397(14) -0.0036(12) 0.0064(11) 0.0068(11) C25 0.0305(12) 0.0309(13) 0.0271(12) 0.0012(10) 0.0023(9) -0.0002(10) C26 0.0324(13) 0.0273(12) 0.0444(15) 0.0026(11) 0.0045(11) -0.0051(10) C26C 0.0399(15) 0.0341(15) 0.070(2) -0.0034(14) 0.0083(14) 0.0026(12) C26B 0.0380(15) 0.0380(15) 0.063(2) -0.0090(14) 0.0038(13) -0.0048(12) C26A 0.0566(19) 0.0463(17) 0.0514(18) 0.0169(15) 0.0129(15) -0.0032(14) C27 0.0451(15) 0.0276(13) 0.0481(16) -0.0027(12) 0.0108(12) 0.0031(11) C27C 0.0572(19) 0.0488(18) 0.0537(19) 0.0148(15) 0.0091(15) 0.0046(15) C27B 0.0545(19) 0.0327(15) 0.080(2) -0.0073(15) 0.0158(17) -0.0080(14) C27A 0.072(2) 0.0439(18) 0.079(3) -0.0193(18) 0.0307(19) 0.0034(16) C110 0.0358(13) 0.0305(13) 0.0300(13) -0.0085(10) 0.0074(10) -0.0003(10) C111 0.0444(16) 0.0445(16) 0.0479(17) -0.0122(14) 0.0153(13) 0.0033(13) C112 0.0444(15) 0.0380(15) 0.0356(14) -0.0100(12) 0.0089(12) -0.0051(12) C113 0.0486(16) 0.0323(14) 0.0421(15) -0.0044(12) 0.0089(12) 0.0012(12) C120 0.0319(13) 0.0335(13) 0.0382(14) -0.0042(11) 0.0159(11) -0.0026(10) C121 0.0384(16) 0.055(2) 0.078(2) -0.0262(18) 0.0234(15) -0.0107(14) C122 0.059(2) 0.061(2) 0.062(2) 0.0138(18) 0.0379(17) 0.0119(17) C123 0.0392(15) 0.0381(15) 0.0619(19) -0.0053(14) 0.0227(14) -0.0026(12) C130 0.0244(12) 0.0423(15) 0.0323(13) -0.0005(11) 0.0038(10) -0.0023(10) C131 0.0309(14) 0.0490(17) 0.0482(17) 0.0011(14) 0.0076(12) 0.0024(12) C132 0.0326(13) 0.0461(16) 0.0383(14) -0.0058(12) 0.0053(11) -0.0063(12) C133 0.0371(15) 0.0533(18) 0.0378(15) 0.0014(13) 0.0021(12) -0.0066(13) C140 0.0358(13) 0.0308(13) 0.0341(13) 0.0031(11) 0.0082(11) 0.0019(10) C141 0.048(6) 0.060(6) 0.045(5) 0.014(4) 0.016(4) 0.003(4) C142 0.074(8) 0.034(4) 0.055(6) 0.014(4) 0.028(6) 0.005(5) C143 0.063(8) 0.040(7) 0.040(5) 0.011(5) -0.012(4) -0.009(5) C144 0.039(6) 0.047(6) 0.037(6) 0.011(4) 0.011(4) 0.007(4) C145 0.095(12) 0.033(5) 0.040(5) 0.004(4) 0.031(8) -0.004(7) C146 0.052(7) 0.045(9) 0.053(8) 0.018(7) 0.004(5) -0.005(7) F11C 0.0555(11) 0.0621(12) 0.0646(12) -0.0287(10) 0.0221(9) 0.0077(9) F11B 0.0385(9) 0.0571(11) 0.0632(12) -0.0150(9) 0.0043(8) 0.0102(8) F11A 0.0480(10) 0.0631(12) 0.0646(12) -0.0034(10) 0.0291(9) -0.0059(9) F12C 0.0628(11) 0.0436(10) 0.0521(10) -0.0204(8) 0.0097(9) -0.0107(8) F12B 0.0644(11) 0.0599(11) 0.0308(8) -0.0056(8) 0.0132(8) -0.0099(9) F12A 0.0369(8) 0.0531(10) 0.0426(9) -0.0062(8) 0.0012(7) -0.0029(7) F13C 0.0643(11) 0.0423(9) 0.0340(8) 0.0015(7) 0.0044(8) 0.0029(8) F13B 0.0771(13) 0.0310(9) 0.0630(12) -0.0013(8) 0.0151(10) 0.0090(8) F13A 0.0508(10) 0.0480(10) 0.0505(10) 0.0043(8) 0.0174(8) -0.0085(8) F21C 0.0333(9) 0.0660(12) 0.1063(17) -0.0301(12) 0.0285(10) -0.0098(8) F21B 0.0384(10) 0.1146(19) 0.0574(12) -0.0377(13) 0.0032(8) -0.0049(10) F21A 0.0630(13) 0.0433(11) 0.146(2) -0.0337(13) 0.0489(14) -0.0208(9) F22C 0.0808(15) 0.0868(16) 0.0880(16) 0.0282(13) 0.0625(13) 0.0174(12) F22B 0.0816(14) 0.0677(13) 0.0795(15) 0.0338(12) 0.0461(12) 0.0260(11) F22A 0.0701(13) 0.1105(19) 0.0399(10) -0.0171(11) 0.0148(9) 0.0091(13) F23C 0.0528(10) 0.0464(10) 0.0697(12) -0.0145(9) 0.0320(9) 0.0025(8) F23B 0.0501(10) 0.0379(9) 0.1090(17) -0.0233(10) 0.0300(11) -0.0111(8) F23A 0.0544(11) 0.0636(12) 0.0720(13) 0.0245(10) 0.0260(10) 0.0209(9) F31C 0.0453(10) 0.0509(11) 0.0631(12) 0.0021(9) 0.0106(8) 0.0131(8) F31B 0.0263(8) 0.0718(13) 0.0707(13) -0.0042(10) 0.0045(8) -0.0042(8) F31A 0.0417(9) 0.0660(12) 0.0531(11) 0.0046(9) 0.0231(8) 0.0077(8) F32C 0.0427(9) 0.0597(11) 0.0478(10) -0.0162(9) 0.0005(8) -0.0123(8) F32B 0.0477(9) 0.0452(10) 0.0546(10) 0.0015(8) 0.0174(8) -0.0105(8) F32A 0.0359(8) 0.0463(9) 0.0521(10) -0.0137(8) 0.0108(7) -0.0015(7) F33C 0.0624(11) 0.0493(10) 0.0483(10) 0.0100(8) 0.0107(8) -0.0097(9) F33B 0.0462(10) 0.0855(14) 0.0409(10) 0.0121(10) -0.0077(8) -0.0068(10) F33A 0.0461(9) 0.0711(12) 0.0342(9) -0.0050(8) 0.0127(7) -0.0096(8) F41A 0.0611(11) 0.0696(13) 0.0484(10) 0.0197(10) 0.0234(9) 0.0057(10) F41B 0.0454(19) 0.083(3) 0.065(2) 0.014(2) 0.0113(17) -0.0203(19) F41C 0.061(4) 0.070(4) 0.061(4) 0.015(3) 0.033(3) 0.024(3) F41D 0.035(3) 0.077(5) 0.047(3) 0.014(3) 0.012(2) 0.008(3) F41E 0.085(4) 0.046(2) 0.040(2) -0.0074(18) 0.022(2) 0.004(2) F42A 0.1002(16) 0.0345(9) 0.0632(12) 0.0118(9) 0.0269(11) 0.0043(10) F42B 0.069(3) 0.052(2) 0.091(3) 0.015(2) 0.040(2) 0.027(2) F42C 0.086(3) 0.038(2) 0.050(3) -0.0068(16) 0.008(3) -0.010(3) F42D 0.099(5) 0.042(3) 0.043(3) -0.004(2) 0.024(4) 0.013(4) F42E 0.088(4) 0.052(3) 0.060(3) -0.001(2) 0.005(3) -0.032(3) F43A 0.0602(12) 0.0676(13) 0.0516(11) 0.0236(10) -0.0050(9) -0.0006(10) F43B 0.045(3) 0.077(4) 0.054(3) 0.006(2) 0.0013(18) -0.016(2) F43C 0.094(3) 0.049(2) 0.0345(17) -0.0038(15) 0.0024(17) -0.0040(19) F43D 0.047(3) 0.052(4) 0.050(4) 0.010(3) -0.008(2) -0.015(3) F43E 0.046(3) 0.099(4) 0.075(3) 0.039(3) 0.025(2) 0.031(3) C200 0.073(3) 0.071(3) 0.087(3) 0.027(2) 0.017(2) -0.006(2) Cl1 0.0576(6) 0.0899(8) 0.1026(8) 0.0387(7) 0.0008(5) 0.0047(5) Cl2 0.0648(5) 0.0702(6) 0.0594(5) 0.0023(4) -0.0091(4) 0.0064(4) C210 0.064(4) 0.044(4) 0.081(5) 0.004(4) 0.025(4) -0.004(3) Cl10 0.199(5) 0.0476(14) 0.112(3) -0.0109(16) 0.070(3) -0.0281(19) Cl11 0.0719(19) 0.130(4) 0.124(4) 0.079(3) 0.016(2) 0.009(2) C220 0.053(6) 0.109(11) 0.150(13) 0.052(10) 0.045(8) 0.012(6) Cl50 0.077(2) 0.176(5) 0.0530(17) 0.010(3) 0.0253(15) 0.032(3) Cl51 0.067(2) 0.084(2) 0.081(2) 0.000(2) 0.0169(16) 0.0045(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ge1 C10 1.893(2) . ? Ge1 C1 1.898(3) . ? Ge1 C20 1.899(2) . ? Al1 O3 1.7255(18) . ? Al1 O4 1.7264(19) . ? Al1 O1 1.7270(18) . ? Al1 O2 1.7280(18) . ? O1 C110 1.352(3) . ? O2 C120 1.353(3) . ? O3 C130 1.356(3) . ? O4 C140 1.358(3) . ? O5 C6 1.372(3) . ? O5 C8 1.471(3) . ? O6 C2 1.369(3) . ? O6 C9 1.470(3) . ? O16 C11 1.363(3) . ? O16 C16 1.475(3) . ? O17 C15 1.360(3) . ? O17 C17 1.467(3) . ? O26 C21 1.371(3) . ? O26 C26 1.468(3) . ? O27 C25 1.369(3) . ? O27 C27 1.469(3) . ? C1 C6 1.395(3) . ? C1 C2 1.397(3) . ? C2 C3 1.384(4) . ? C3 C4 1.394(4) . ? C4 C5 1.387(4) . ? C5 C6 1.382(4) . ? C8C C8 1.515(5) . ? C8 C8B 1.507(5) . ? C8 C8A 1.518(4) . ? C9C C9 1.519(4) . ? C9B C9 1.519(4) . ? C9A C9 1.519(4) . ? C10 C11 1.398(4) . ? C10 C15 1.399(4) . ? C11 C12 1.386(4) . ? C12 C13 1.389(4) . ? C13 C14 1.383(4) . ? C14 C15 1.388(4) . ? C16C C16 1.529(4) . ? C16 C16A 1.511(4) . ? C16 C16B 1.514(5) . ? C17A C17 1.523(4) . ? C17 C17C 1.511(4) . ? C17 C17B 1.526(4) . ? C20 C25 1.390(3) . ? C20 C21 1.393(3) . ? C21 C22 1.385(3) . ? C22 C23 1.387(4) . ? C23 C24 1.389(4) . ? C24 C25 1.395(4) . ? C26 C26A 1.510(4) . ? C26 C26C 1.510(4) . ? C26 C26B 1.526(4) . ? C27 C27B 1.513(4) . ? C27 C27C 1.522(4) . ? C27 C27A 1.524(4) . ? C110 C113 1.544(4) . ? C110 C112 1.556(4) . ? C110 C111 1.557(4) . ? C111 F11A 1.323(4) . ? C111 F11B 1.331(4) . ? C111 F11C 1.346(3) . ? C112 F12A 1.321(3) . ? C112 F12C 1.338(3) . ? C112 F12B 1.343(3) . ? C113 F13B 1.330(3) . ? C113 F13A 1.335(3) . ? C113 F13C 1.339(3) . ? C120 C121 1.536(4) . ? C120 C123 1.549(4) . ? C120 C122 1.559(4) . ? C121 F21B 1.324(4) . ? C121 F21C 1.339(3) . ? C121 F21A 1.348(4) . ? C122 F22B 1.325(4) . ? C122 F22A 1.327(5) . ? C122 F22C 1.343(4) . ? C123 F23B 1.320(3) . ? C123 F23C 1.335(3) . ? C123 F23A 1.339(4) . ? C130 C131 1.545(4) . ? C130 C132 1.554(4) . ? C130 C133 1.555(4) . ? C131 F31A 1.330(4) . ? C131 F31C 1.334(4) . ? C131 F31B 1.340(3) . ? C132 F32A 1.327(3) . ? C132 F32B 1.341(3) . ? C132 F32C 1.341(3) . ? C133 F33B 1.329(3) . ? C133 F33A 1.332(4) . ? C133 F33C 1.335(4) . ? C140 C146 1.53(2) . ? C140 C141 1.544(12) . ? C140 C145 1.547(17) . ? C140 C142 1.548(15) . ? C140 C143 1.552(17) . ? C140 C144 1.569(13) . ? C141 F41B 1.297(10) . ? C141 F41C 1.342(14) . ? C141 F41A 1.377(10) . ? C142 F42C 1.319(18) . ? C142 F42B 1.320(12) . ? C142 F42A 1.400(13) . ? C143 F43B 1.31(2) . ? C143 F43C 1.328(13) . ? C143 F43A 1.357(16) . ? C144 F41A 1.287(12) . ? C144 F41D 1.316(14) . ? C144 F41E 1.387(12) . ? C145 F42A 1.270(18) . ? C145 F42D 1.311(17) . ? C145 F42E 1.374(17) . ? C146 F43A 1.27(2) . ? C146 F43D 1.35(2) . ? C146 F43E 1.391(19) . ? C200 Cl1 1.722(4) . ? C200 Cl2 1.749(4) . ? C210 Cl11 1.778(10) 3_667 ? C210 Cl10 1.861(11) 3_667 ? Cl10 C210 1.861(11) 3_667 ? Cl11 C210 1.778(10) 3_667 ? C220 Cl50 1.691(18) . ? C220 Cl51 1.694(16) 3_566 ? C220 Cl50 2.065(14) 3_566 ? Cl50 Cl51 0.780(6) . ? Cl50 C220 2.065(14) 3_566 ? Cl51 C220 1.694(16) 3_566 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C10 Ge1 C1 121.01(10) . . ? C10 Ge1 C20 117.79(10) . . ? C1 Ge1 C20 121.19(10) . . ? O3 Al1 O4 112.72(9) . . ? O3 Al1 O1 107.15(9) . . ? O4 Al1 O1 107.87(9) . . ? O3 Al1 O2 108.07(9) . . ? O4 Al1 O2 108.28(9) . . ? O1 Al1 O2 112.84(9) . . ? C110 O1 Al1 147.20(17) . . ? C120 O2 Al1 148.47(18) . . ? C130 O3 Al1 145.86(17) . . ? C140 O4 Al1 147.15(17) . . ? C6 O5 C8 124.5(2) . . ? C2 O6 C9 124.18(19) . . ? C11 O16 C16 124.9(2) . . ? C15 O17 C17 124.5(2) . . ? C21 O26 C26 123.93(19) . . ? C25 O27 C27 122.79(19) . . ? C6 C1 C2 121.2(2) . . ? C6 C1 Ge1 119.11(19) . . ? C2 C1 Ge1 119.66(18) . . ? O6 C2 C3 128.1(2) . . ? O6 C2 C1 112.2(2) . . ? C3 C2 C1 119.6(2) . . ? C2 C3 C4 118.3(2) . . ? C5 C4 C3 122.7(3) . . ? C6 C5 C4 118.6(2) . . ? O5 C6 C5 128.2(2) . . ? O5 C6 C1 112.2(2) . . ? C5 C6 C1 119.5(2) . . ? O5 C8 C8B 109.9(3) . . ? O5 C8 C8C 101.3(2) . . ? C8B C8 C8C 111.5(3) . . ? O5 C8 C8A 110.4(3) . . ? C8B C8 C8A 113.3(3) . . ? C8C C8 C8A 109.8(3) . . ? O6 C9 C9B 110.2(2) . . ? O6 C9 C9C 101.8(2) . . ? C9B C9 C9C 110.0(2) . . ? O6 C9 C9A 111.0(2) . . ? C9B C9 C9A 113.5(2) . . ? C9C C9 C9A 109.6(2) . . ? C11 C10 C15 121.4(2) . . ? C11 C10 Ge1 119.63(18) . . ? C15 C10 Ge1 118.86(18) . . ? O16 C11 C12 128.5(2) . . ? O16 C11 C10 112.3(2) . . ? C12 C11 C10 119.2(2) . . ? C11 C12 C13 118.6(3) . . ? C14 C13 C12 123.0(3) . . ? C13 C14 C15 118.6(3) . . ? O17 C15 C14 127.8(2) . . ? O17 C15 C10 112.9(2) . . ? C14 C15 C10 119.2(2) . . ? O16 C16 C16A 102.3(2) . . ? O16 C16 C16B 110.1(2) . . ? C16A C16 C16B 110.7(3) . . ? O16 C16 C16C 110.3(2) . . ? C16A C16 C16C 109.6(3) . . ? C16B C16 C16C 113.3(3) . . ? O17 C17 C17C 110.8(2) . . ? O17 C17 C17A 110.8(2) . . ? C17C C17 C17A 112.3(3) . . ? O17 C17 C17B 101.9(2) . . ? C17C C17 C17B 111.6(3) . . ? C17A C17 C17B 109.0(3) . . ? C25 C20 C21 121.5(2) . . ? C25 C20 Ge1 119.26(18) . . ? C21 C20 Ge1 119.01(18) . . ? O26 C21 C22 127.9(2) . . ? O26 C21 C20 112.5(2) . . ? C22 C21 C20 119.5(2) . . ? C21 C22 C23 118.6(2) . . ? C22 C23 C24 122.7(2) . . ? C23 C24 C25 118.3(2) . . ? O27 C25 C20 113.1(2) . . ? O27 C25 C24 127.2(2) . . ? C20 C25 C24 119.3(2) . . ? O26 C26 C26A 109.7(2) . . ? O26 C26 C26C 102.0(2) . . ? C26A C26 C26C 111.5(3) . . ? O26 C26 C26B 110.4(2) . . ? C26A C26 C26B 113.3(2) . . ? C26C C26 C26B 109.3(2) . . ? O27 C27 C27B 102.0(2) . . ? O27 C27 C27C 109.3(2) . . ? C27B C27 C27C 111.0(3) . . ? O27 C27 C27A 110.1(3) . . ? C27B C27 C27A 109.6(3) . . ? C27C C27 C27A 114.2(3) . . ? O1 C110 C113 111.2(2) . . ? O1 C110 C112 107.3(2) . . ? C113 C110 C112 109.1(2) . . ? O1 C110 C111 110.6(2) . . ? C113 C110 C111 109.4(2) . . ? C112 C110 C111 109.1(2) . . ? F11A C111 F11B 107.5(2) . . ? F11A C111 F11C 107.7(2) . . ? F11B C111 F11C 106.6(2) . . ? F11A C111 C110 111.4(2) . . ? F11B C111 C110 111.2(2) . . ? F11C C111 C110 112.1(2) . . ? F12A C112 F12C 108.0(2) . . ? F12A C112 F12B 107.4(2) . . ? F12C C112 F12B 106.8(2) . . ? F12A C112 C110 111.2(2) . . ? F12C C112 C110 112.4(2) . . ? F12B C112 C110 110.8(2) . . ? F13B C113 F13A 107.3(2) . . ? F13B C113 F13C 107.2(2) . . ? F13A C113 F13C 107.4(2) . . ? F13B C113 C110 112.9(2) . . ? F13A C113 C110 111.3(2) . . ? F13C C113 C110 110.5(2) . . ? O2 C120 C121 111.0(2) . . ? O2 C120 C123 111.1(2) . . ? C121 C120 C123 109.4(2) . . ? O2 C120 C122 107.6(2) . . ? C121 C120 C122 109.7(3) . . ? C123 C120 C122 108.0(2) . . ? F21B C121 F21C 107.6(3) . . ? F21B C121 F21A 107.2(3) . . ? F21C C121 F21A 107.0(3) . . ? F21B C121 C120 111.1(3) . . ? F21C C121 C120 113.5(3) . . ? F21A C121 C120 110.2(3) . . ? F22B C122 F22A 107.7(3) . . ? F22B C122 F22C 107.2(3) . . ? F22A C122 F22C 108.0(3) . . ? F22B C122 C120 110.7(3) . . ? F22A C122 C120 111.3(3) . . ? F22C C122 C120 111.6(3) . . ? F23B C123 F23C 108.6(2) . . ? F23B C123 F23A 107.1(3) . . ? F23C C123 F23A 106.8(2) . . ? F23B C123 C120 110.7(2) . . ? F23C C123 C120 112.7(2) . . ? F23A C123 C120 110.7(2) . . ? O3 C130 C131 107.9(2) . . ? O3 C130 C132 110.4(2) . . ? C131 C130 C132 108.8(2) . . ? O3 C130 C133 110.9(2) . . ? C131 C130 C133 109.7(2) . . ? C132 C130 C133 109.0(2) . . ? F31A C131 F31C 107.5(3) . . ? F31A C131 F31B 107.3(2) . . ? F31C C131 F31B 107.3(2) . . ? F31A C131 C130 111.2(2) . . ? F31C C131 C130 110.6(2) . . ? F31B C131 C130 112.7(2) . . ? F32A C132 F32B 107.5(2) . . ? F32A C132 F32C 107.5(2) . . ? F32B C132 F32C 107.2(2) . . ? F32A C132 C130 110.9(2) . . ? F32B C132 C130 110.6(2) . . ? F32C C132 C130 113.0(2) . . ? F33B C133 F33A 107.5(2) . . ? F33B C133 F33C 107.9(3) . . ? F33A C133 F33C 107.2(2) . . ? F33B C133 C130 112.6(2) . . ? F33A C133 C130 111.2(2) . . ? F33C C133 C130 110.2(2) . . ? O4 C140 C146 112.2(9) . . ? O4 C140 C141 109.2(4) . . ? C146 C140 C141 125.7(9) . . ? O4 C140 C145 110.8(7) . . ? C146 C140 C145 107.5(9) . . ? C141 C140 C145 88.4(6) . . ? O4 C140 C142 105.4(6) . . ? C146 C140 C142 91.6(8) . . ? C141 C140 C142 109.6(6) . . ? C145 C140 C142 21.6(6) . . ? O4 C140 C143 108.8(7) . . ? C146 C140 C143 19.7(7) . . ? C141 C140 C143 112.6(8) . . ? C145 C140 C143 124.9(8) . . ? C142 C140 C143 110.8(7) . . ? O4 C140 C144 112.7(5) . . ? C146 C140 C144 106.2(9) . . ? C141 C140 C144 22.9(4) . . ? C145 C140 C144 107.1(7) . . ? C142 C140 C144 126.7(6) . . ? C143 C140 C144 90.7(8) . . ? F41B C141 F41C 109.2(9) . . ? F41B C141 F41A 106.5(7) . . ? F41C C141 F41A 106.6(8) . . ? F41B C141 C140 112.9(8) . . ? F41C C141 C140 110.0(7) . . ? F41A C141 C140 111.4(7) . . ? F42C C142 F42B 108.8(12) . . ? F42C C142 F42A 109.3(9) . . ? F42B C142 F42A 105.6(10) . . ? F42C C142 C140 112.8(10) . . ? F42B C142 C140 111.6(9) . . ? F42A C142 C140 108.5(10) . . ? F43B C143 F43C 110.2(12) . . ? F43B C143 F43A 111.0(12) . . ? F43C C143 F43A 102.9(12) . . ? F43B C143 C140 110.8(12) . . ? F43C C143 C140 110.4(11) . . ? F43A C143 C140 111.3(11) . . ? F41A C144 F41D 110.4(10) . . ? F41A C144 F41E 104.9(8) . . ? F41D C144 F41E 106.7(10) . . ? F41A C144 C140 115.1(9) . . ? F41D C144 C140 110.8(8) . . ? F41E C144 C140 108.6(8) . . ? F42A C145 F42D 108.1(13) . . ? F42A C145 F42E 107.6(10) . . ? F42D C145 F42E 106.8(13) . . ? F42A C145 C140 116.0(13) . . ? F42D C145 C140 110.0(10) . . ? F42E C145 C140 107.9(12) . . ? F43A C146 F43D 109.8(17) . . ? F43A C146 F43E 103.2(12) . . ? F43D C146 F43E 104.0(15) . . ? F43A C146 C140 118.3(17) . . ? F43D C146 C140 111.0(12) . . ? F43E C146 C140 109.4(14) . . ? C144 F41A C141 26.6(4) . . ? C145 F42A C142 24.4(8) . . ? C146 F43A C143 22.9(10) . . ? Cl1 C200 Cl2 113.1(2) . . ? Cl11 C210 Cl10 12.3(3) 3_667 3_667 ? Cl50 C220 Cl51 115.7(8) . 3_566 ? Cl50 C220 Cl50 94.9(7) . 3_566 ? Cl51 C220 Cl50 21.1(2) 3_566 3_566 ? Cl51 Cl50 C220 135.7(8) . . ? Cl51 Cl50 C220 51.6(8) . 3_566 ? C220 Cl50 C220 85.1(7) . 3_566 ? Cl50 Cl51 C220 107.3(9) . 3_566 ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 26.06 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.786 _refine_diff_density_min -0.486 _refine_diff_density_rms 0.056 # Attachment 'CS70P-1.CIF' data_cs70p-1 _database_code_depnum_ccdc_archive 'CCDC 698440' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H64 Ge O7' _chemical_formula_weight 753.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.869(2) _cell_length_b 12.774(3) _cell_length_c 13.757(3) _cell_angle_alpha 90.70(3) _cell_angle_beta 95.43(3) _cell_angle_gamma 90.95(3) _cell_volume 2075.9(7) _cell_formula_units_Z 2 _cell_measurement_temperature 149(2) _cell_measurement_reflns_used 25423 _cell_measurement_theta_min 1.44 _cell_measurement_theta_max 25.94 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.205 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 0.783 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7874 _exptl_absorpt_correction_T_max 0.8745 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 149(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14158 _diffrn_reflns_av_R_equivalents 0.0667 _diffrn_reflns_av_sigmaI/netI 0.0836 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 26.05 _reflns_number_total 7372 _reflns_number_gt 5339 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0596P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7372 _refine_ls_number_parameters 498 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0725 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1179 _refine_ls_wR_factor_gt 0.1076 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.947 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ge1 Ge 0.28617(3) 0.79509(3) 0.28317(3) 0.03019(12) Uani 0.9479(14) 1 d P A 1 O100 O 0.32367(19) 0.88158(18) 0.38487(17) 0.0358(6) Uani 0.9479(14) 1 d P A 1 Ge1A Ge 0.2725(6) 0.7296(6) 0.2187(6) 0.047(3) Uiso 0.0521(14) 1 d P A 2 O101 O 0.237(4) 0.631(4) 0.125(4) 0.049(11) Uiso 0.0521(14) 1 d P A 2 O1 O 0.4143(2) 0.58681(16) 0.24485(18) 0.0446(6) Uani 1 1 d . . . O2 O 0.1377(2) 0.72723(16) 0.42663(17) 0.0422(6) Uani 1 1 d . . . O10 O 0.06642(19) 0.67457(16) 0.20781(19) 0.0464(6) Uani 1 1 d . . . O11 O 0.21584(19) 1.01525(17) 0.25067(18) 0.0456(6) Uani 1 1 d . . . O20 O 0.53142(19) 0.78364(17) 0.33296(17) 0.0415(6) Uani 1 1 d . . . O21 O 0.2776(2) 0.85110(17) 0.05381(17) 0.0426(6) Uani 1 1 d . . . C1 C 0.2825(3) 0.6572(2) 0.3422(3) 0.0369(8) Uani 1 1 d . . . C2 C 0.2075(3) 0.6451(2) 0.4144(3) 0.0443(9) Uani 1 1 d . A . C3 C 0.1992(3) 0.5507(3) 0.4639(3) 0.0546(10) Uani 1 1 d . . . H3A H 0.1485 0.5433 0.5130 0.066 Uiso 1 1 calc R A . C4 C 0.2654(4) 0.4687(3) 0.4404(3) 0.0604(11) Uani 1 1 d . A . H4A H 0.2608 0.4047 0.4743 0.073 Uiso 1 1 calc R . . C6 C 0.3384(3) 0.4772(3) 0.3687(3) 0.0514(10) Uani 1 1 d . . . H6A H 0.3826 0.4191 0.3530 0.062 Uiso 1 1 calc R A . C5 C 0.3473(3) 0.5716(2) 0.3189(3) 0.0413(8) Uani 1 1 d . A . C7C C 0.4364(4) 0.4176(3) 0.1654(4) 0.0758(14) Uani 1 1 d . . . H7CA H 0.375(3) 0.4408(7) 0.117(2) 0.114 Uiso 1 1 calc R . . H7CB H 0.404(3) 0.3739(19) 0.2151(14) 0.114 Uiso 1 1 calc R . . H7CC H 0.4912(17) 0.3761(19) 0.132(2) 0.114 Uiso 1 1 calc R . . C7 C 0.4967(3) 0.5130(3) 0.2149(3) 0.0485(9) Uani 1 1 d . . . C7B C 0.5569(3) 0.5731(3) 0.1410(3) 0.0598(11) Uani 1 1 d . . . H7BA H 0.5006(14) 0.598(2) 0.0890(16) 0.090 Uiso 1 1 calc R . . H7BB H 0.611(2) 0.5267(13) 0.1116(17) 0.090 Uiso 1 1 calc R . . H7BC H 0.598(2) 0.6338(19) 0.1736(9) 0.090 Uiso 1 1 calc R . . C7A C 0.5827(4) 0.4863(4) 0.3012(4) 0.0831(17) Uani 1 1 d . . . H7AA H 0.618(3) 0.5527(19) 0.331(2) 0.125 Uiso 1 1 calc R . . H7AB H 0.643(2) 0.441(3) 0.2774(9) 0.125 Uiso 1 1 calc R . . H7AC H 0.5431(13) 0.447(3) 0.3515(19) 0.125 Uiso 1 1 calc R . . C8 C 0.1139(3) 0.7684(3) 0.5214(3) 0.0494(9) Uani 1 1 d . . . C8C C 0.0740(4) 0.8782(3) 0.4984(3) 0.0561(10) Uani 1 1 d . . . H8CA H 0.010(2) 0.8748(3) 0.4467(19) 0.084 Uiso 1 1 calc R . . H8CB H 0.1371(16) 0.9202(12) 0.475(2) 0.084 Uiso 1 1 calc R . . H8CC H 0.049(2) 0.9115(11) 0.5582(15) 0.084 Uiso 1 1 calc R . . C8B C 0.0180(4) 0.7054(3) 0.5609(4) 0.0700(13) Uani 1 1 d . . . H8BA H -0.050(2) 0.696(2) 0.5059(15) 0.105 Uiso 1 1 calc R . . H8BB H -0.0100(19) 0.7453(15) 0.622(2) 0.105 Uiso 1 1 calc R . . H8BC H 0.0476(11) 0.631(2) 0.583(2) 0.105 Uiso 1 1 calc R . . C8A C 0.2201(4) 0.7716(3) 0.5923(3) 0.0671(13) Uani 1 1 d . . . H8AA H 0.2825(18) 0.807(2) 0.5613(12) 0.101 Uiso 1 1 calc R . . H8AB H 0.2425(18) 0.6988(19) 0.6094(19) 0.101 Uiso 1 1 calc R . . H8AC H 0.2049(9) 0.811(2) 0.6526(18) 0.101 Uiso 1 1 calc R . . C10 C 0.1364(3) 0.8450(2) 0.2327(2) 0.0337(7) Uani 1 1 d . . . C11 C 0.1197(3) 0.9524(2) 0.2299(2) 0.0378(8) Uani 1 1 d . A . C12 C 0.0124(3) 0.9943(3) 0.2149(3) 0.0478(9) Uani 1 1 d . . . H12A H 0.0025 1.0679 0.2169 0.057 Uiso 1 1 calc R A . C13 C -0.0796(3) 0.9268(3) 0.1971(3) 0.0495(10) Uani 1 1 d . A . H13A H -0.1535 0.9546 0.1866 0.059 Uiso 1 1 calc R . . C14 C -0.0661(3) 0.8200(3) 0.1942(3) 0.0464(9) Uani 1 1 d . . . H14A H -0.1301 0.7748 0.1799 0.056 Uiso 1 1 calc R A . C15 C 0.0408(3) 0.7786(2) 0.2122(2) 0.0375(8) Uani 1 1 d . A . C17 C -0.0165(3) 0.5882(3) 0.1955(3) 0.0541(10) Uani 1 1 d . . . C17C C 0.0602(4) 0.4933(3) 0.2006(4) 0.0632(12) Uani 1 1 d . . . H17A H 0.101(2) 0.4909(14) 0.2638(18) 0.095 Uiso 1 1 calc R . . H17B H 0.112(2) 0.4987(12) 0.1519(19) 0.095 Uiso 1 1 calc R . . H17C H 0.0151(12) 0.4308(16) 0.189(2) 0.095 Uiso 1 1 calc R . . C17B C -0.0825(4) 0.5930(3) 0.0944(4) 0.0747(15) Uani 1 1 d . . . H17D H -0.140(2) 0.649(2) 0.0944(8) 0.112 Uiso 1 1 calc R . . H17E H -0.121(3) 0.525(2) 0.0786(12) 0.112 Uiso 1 1 calc R . . H17F H -0.0293(15) 0.609(3) 0.0447(14) 0.112 Uiso 1 1 calc R . . C17A C -0.0911(4) 0.5874(3) 0.2789(4) 0.0699(13) Uani 1 1 d . . . H17G H -0.137(2) 0.649(2) 0.2761(13) 0.105 Uiso 1 1 calc R . . H17H H -0.0443(12) 0.587(2) 0.3401(16) 0.105 Uiso 1 1 calc R . . H17I H -0.139(2) 0.526(2) 0.2735(13) 0.105 Uiso 1 1 calc R . . C18 C 0.2378(3) 1.1101(2) 0.1961(3) 0.0436(9) Uani 1 1 d . . . C18C C 0.1895(3) 1.1002(3) 0.0895(3) 0.0506(10) Uani 1 1 d . . . H18A H 0.1072(19) 1.098(2) 0.0859(3) 0.076 Uiso 1 1 calc R . . H18B H 0.2158(18) 1.0358(18) 0.0613(9) 0.076 Uiso 1 1 calc R . . H18C H 0.2147(18) 1.1598(17) 0.0534(10) 0.076 Uiso 1 1 calc R . . C18B C 0.3670(3) 1.1148(3) 0.2033(3) 0.0495(9) Uani 1 1 d . . . H18D H 0.3969 1.1209 0.2720 0.074 Uiso 1 1 calc R . . H18E H 0.3919 1.1757 0.1678 0.074 Uiso 1 1 calc R . . H18F H 0.3951 1.0508 0.1747 0.074 Uiso 1 1 calc R . . C18A C 0.1913(3) 1.2048(3) 0.2459(3) 0.0552(10) Uani 1 1 d . . . H18G H 0.2176(19) 1.2040(11) 0.3198(17) 0.083 Uiso 1 1 calc R . . H18H H 0.104(2) 1.2023(11) 0.2361(16) 0.083 Uiso 1 1 calc R . . H18I H 0.2209(19) 1.2725(16) 0.2158(15) 0.083 Uiso 1 1 calc R . . C20 C 0.4058(3) 0.8185(2) 0.1953(2) 0.0333(7) Uani 1 1 d . . . C21 C 0.5171(3) 0.8216(2) 0.2390(2) 0.0379(8) Uani 1 1 d . A . C22 C 0.6062(3) 0.8529(3) 0.1884(3) 0.0461(9) Uani 1 1 d . . . H22A H 0.6810 0.8551 0.2197 0.055 Uiso 1 1 calc R A . C23 C 0.5859(3) 0.8812(3) 0.0919(3) 0.0489(9) Uani 1 1 d . A . H23A H 0.6472 0.9036 0.0571 0.059 Uiso 1 1 calc R . . C24 C 0.4779(3) 0.8771(3) 0.0457(3) 0.0463(9) Uani 1 1 d . . . H24A H 0.4646 0.8961 -0.0209 0.056 Uiso 1 1 calc R A . C25 C 0.3883(3) 0.8451(2) 0.0971(2) 0.0379(8) Uani 1 1 d . A . C27 C 0.6055(3) 0.8361(3) 0.4110(3) 0.0462(9) Uani 1 1 d . . . C27C C 0.5996(3) 0.9536(3) 0.4046(3) 0.0569(11) Uani 1 1 d . . . H27A H 0.517(2) 0.9756(6) 0.400(2) 0.085 Uiso 1 1 calc R . . H27B H 0.635(2) 0.9779(7) 0.3438(18) 0.085 Uiso 1 1 calc R . . H27C H 0.643(2) 0.9870(9) 0.4655(17) 0.085 Uiso 1 1 calc R . . C27B C 0.5567(3) 0.7967(3) 0.5014(3) 0.0584(11) Uani 1 1 d . . . H27D H 0.478(2) 0.8196(19) 0.5015(10) 0.088 Uiso 1 1 calc R . . H27E H 0.6017(17) 0.8247(18) 0.5596(14) 0.088 Uiso 1 1 calc R . . H27F H 0.558(2) 0.7200(18) 0.5018(10) 0.088 Uiso 1 1 calc R . . C27A C 0.7280(3) 0.7991(3) 0.4088(3) 0.0614(12) Uani 1 1 d . . . H27G H 0.7640(12) 0.8358(18) 0.3555(18) 0.092 Uiso 1 1 calc R . . H27H H 0.7277(3) 0.7218(19) 0.396(2) 0.092 Uiso 1 1 calc R . . H27I H 0.7718(13) 0.816(2) 0.4730(17) 0.092 Uiso 1 1 calc R . . C28C C 0.2521(4) 0.6640(3) 0.0233(4) 0.0704(14) Uani 1 1 d . . . H28A H 0.336(2) 0.6529(11) 0.045(2) 0.106 Uiso 1 1 calc R . . H28B H 0.224(3) 0.6086(15) -0.0276(15) 0.106 Uiso 1 1 calc R . . H28C H 0.207(2) 0.6580(9) 0.082(2) 0.106 Uiso 1 1 calc R . . C28B C 0.1130(3) 0.7987(4) -0.0389(3) 0.0633(12) Uani 1 1 d . . . H28D H 0.1053(4) 0.8768(19) -0.064(2) 0.095 Uiso 1 1 calc R . . H28E H 0.0737(11) 0.791(2) 0.0269(16) 0.095 Uiso 1 1 calc R . . H28F H 0.0729(12) 0.7465(19) -0.0926(19) 0.095 Uiso 1 1 calc R . . C28 C 0.2371(3) 0.7724(3) -0.0205(3) 0.0513(10) Uani 1 1 d . . . C28A C 0.2951(4) 0.7844(4) -0.1127(3) 0.0759(14) Uani 1 1 d . . . H28G H 0.289(2) 0.861(2) -0.1358(15) 0.114 Uiso 1 1 calc R . . H28H H 0.256(2) 0.735(2) -0.1667(16) 0.114 Uiso 1 1 calc R . . H28I H 0.380(2) 0.765(2) -0.0992(7) 0.114 Uiso 1 1 calc R . . H100 H 0.300(3) 0.936(3) 0.370(2) 0.031(9) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ge1 0.03070(19) 0.03056(18) 0.0299(2) 0.00403(13) 0.00601(14) -0.00236(12) O100 0.0363(13) 0.0341(12) 0.0377(15) 0.0011(10) 0.0068(11) 0.0016(10) O1 0.0522(15) 0.0332(11) 0.0507(16) 0.0059(10) 0.0151(13) 0.0026(10) O2 0.0478(14) 0.0434(12) 0.0376(14) 0.0080(10) 0.0140(12) 0.0057(10) O10 0.0382(13) 0.0391(12) 0.0614(17) -0.0049(11) 0.0046(12) -0.0089(9) O11 0.0376(13) 0.0425(12) 0.0564(17) 0.0164(11) 0.0027(12) -0.0083(10) O20 0.0399(13) 0.0465(12) 0.0382(14) 0.0054(10) 0.0043(11) -0.0061(10) O21 0.0444(14) 0.0495(13) 0.0339(14) 0.0044(10) 0.0041(11) 0.0025(10) C1 0.0337(17) 0.0405(17) 0.037(2) 0.0045(13) 0.0028(15) -0.0030(13) C2 0.048(2) 0.0383(17) 0.047(2) 0.0079(15) 0.0066(18) 0.0013(14) C3 0.065(3) 0.046(2) 0.058(3) 0.0235(17) 0.030(2) 0.0062(17) C4 0.073(3) 0.0434(19) 0.069(3) 0.0272(19) 0.023(2) 0.0080(18) C6 0.059(2) 0.0382(18) 0.060(3) 0.0142(16) 0.017(2) 0.0056(16) C5 0.047(2) 0.0368(17) 0.041(2) 0.0066(14) 0.0082(17) -0.0030(14) C7C 0.092(4) 0.053(2) 0.087(4) -0.020(2) 0.041(3) -0.012(2) C7 0.048(2) 0.0370(17) 0.063(3) 0.0051(16) 0.017(2) 0.0044(15) C7B 0.053(2) 0.055(2) 0.077(3) 0.008(2) 0.034(2) 0.0081(18) C7A 0.051(3) 0.096(3) 0.102(4) 0.039(3) 0.003(3) 0.013(2) C8 0.054(2) 0.053(2) 0.044(2) 0.0078(16) 0.0183(19) 0.0014(16) C8C 0.065(3) 0.049(2) 0.058(3) 0.0064(17) 0.023(2) 0.0128(18) C8B 0.077(3) 0.067(3) 0.074(3) 0.018(2) 0.046(3) 0.005(2) C8A 0.079(3) 0.075(3) 0.046(3) 0.003(2) 0.000(2) 0.012(2) C10 0.0354(17) 0.0384(16) 0.0288(18) 0.0067(13) 0.0102(15) -0.0024(12) C11 0.0370(18) 0.0423(17) 0.0350(19) 0.0090(14) 0.0079(15) -0.0058(13) C12 0.0397(19) 0.0444(18) 0.060(3) 0.0163(16) 0.0072(18) 0.0002(14) C13 0.0326(18) 0.054(2) 0.063(3) 0.0168(18) 0.0078(18) 0.0021(15) C14 0.0347(18) 0.049(2) 0.055(2) 0.0054(16) 0.0021(18) -0.0056(14) C15 0.0363(18) 0.0411(17) 0.035(2) 0.0025(13) 0.0050(15) -0.0025(13) C17 0.050(2) 0.0456(19) 0.067(3) -0.0024(18) 0.008(2) -0.0162(16) C17C 0.062(3) 0.042(2) 0.085(3) -0.0044(19) 0.009(2) -0.0105(17) C17B 0.072(3) 0.067(3) 0.080(4) -0.014(2) -0.014(3) -0.017(2) C17A 0.065(3) 0.058(2) 0.090(4) 0.013(2) 0.028(3) -0.012(2) C18 0.045(2) 0.0335(16) 0.053(2) 0.0078(15) 0.0125(18) -0.0042(14) C18C 0.054(2) 0.054(2) 0.046(2) 0.0173(17) 0.0161(19) 0.0022(16) C18B 0.043(2) 0.0409(18) 0.067(3) 0.0043(17) 0.0173(19) -0.0060(14) C18A 0.059(2) 0.0414(19) 0.066(3) 0.0000(18) 0.012(2) 0.0007(16) C20 0.0337(17) 0.0307(15) 0.0375(19) 0.0037(13) 0.0130(15) -0.0010(12) C21 0.0413(19) 0.0382(16) 0.035(2) 0.0044(13) 0.0083(16) -0.0047(13) C22 0.0370(19) 0.058(2) 0.044(2) 0.0058(16) 0.0106(17) -0.0089(15) C23 0.046(2) 0.058(2) 0.046(2) 0.0072(17) 0.0231(19) -0.0074(16) C24 0.051(2) 0.0513(19) 0.037(2) 0.0085(15) 0.0097(18) -0.0089(16) C25 0.0398(18) 0.0392(16) 0.035(2) 0.0038(13) 0.0075(16) -0.0039(13) C27 0.045(2) 0.054(2) 0.039(2) 0.0022(15) -0.0015(17) -0.0035(15) C27C 0.054(2) 0.056(2) 0.059(3) -0.0133(18) 0.000(2) -0.0091(17) C27B 0.053(2) 0.081(3) 0.041(2) 0.0048(19) 0.004(2) 0.006(2) C27A 0.040(2) 0.086(3) 0.058(3) 0.013(2) 0.003(2) 0.0009(19) C28C 0.069(3) 0.049(2) 0.088(4) -0.009(2) -0.017(3) -0.0026(19) C28B 0.052(2) 0.087(3) 0.049(3) 0.000(2) -0.001(2) 0.005(2) C28 0.049(2) 0.056(2) 0.047(2) -0.0060(17) -0.0028(19) 0.0013(16) C28A 0.073(3) 0.107(4) 0.047(3) -0.015(2) 0.010(3) -0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ge1 O100 1.790(2) . ? Ge1 C1 1.950(3) . ? Ge1 C10 1.965(3) . ? Ge1 C20 1.971(3) . ? Ge1A O101 1.81(5) . ? Ge1A C1 1.939(8) . ? Ge1A C20 1.985(8) . ? Ge1A C10 2.225(8) . ? O1 C5 1.364(4) . ? O1 C7 1.454(4) . ? O2 C2 1.366(4) . ? O2 C8 1.453(5) . ? O10 C15 1.370(4) . ? O10 C17 1.464(4) . ? O11 C11 1.389(4) . ? O11 C18 1.466(4) . ? O20 C21 1.383(4) . ? O20 C27 1.470(4) . ? O21 C25 1.394(4) . ? O21 C28 1.467(4) . ? C1 C5 1.399(5) . ? C1 C2 1.403(5) . ? C2 C3 1.400(4) . ? C3 C4 1.373(6) . ? C4 C6 1.377(6) . ? C6 C5 1.402(4) . ? C7C C7 1.522(5) . ? C7 C7B 1.508(5) . ? C7 C7A 1.535(6) . ? C8 C8C 1.515(5) . ? C8 C8A 1.518(6) . ? C8 C8B 1.529(5) . ? C10 C11 1.390(4) . ? C10 C15 1.410(4) . ? C11 C12 1.389(5) . ? C12 C13 1.382(5) . ? C13 C14 1.377(5) . ? C14 C15 1.385(5) . ? C17 C17A 1.513(6) . ? C17 C17C 1.527(5) . ? C17 C17B 1.532(6) . ? C18 C18A 1.521(5) . ? C18 C18C 1.525(5) . ? C18 C18B 1.527(5) . ? C20 C25 1.395(5) . ? C20 C21 1.398(4) . ? C21 C22 1.376(5) . ? C22 C23 1.380(5) . ? C23 C24 1.376(5) . ? C24 C25 1.390(5) . ? C27 C27C 1.507(5) . ? C27 C27B 1.510(5) . ? C27 C27A 1.538(5) . ? C28C C28 1.523(5) . ? C28B C28 1.516(5) . ? C28 C28A 1.508(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O100 Ge1 C1 103.67(13) . . ? O100 Ge1 C10 102.61(12) . . ? C1 Ge1 C10 113.81(13) . . ? O100 Ge1 C20 104.50(12) . . ? C1 Ge1 C20 115.76(14) . . ? C10 Ge1 C20 114.37(13) . . ? O101 Ge1A C1 106.2(16) . . ? O101 Ge1A C20 114.0(17) . . ? C1 Ge1A C20 115.6(4) . . ? O101 Ge1A C10 113.5(15) . . ? C1 Ge1A C10 103.8(4) . . ? C20 Ge1A C10 103.4(3) . . ? C5 O1 C7 125.0(3) . . ? C2 O2 C8 123.9(3) . . ? C15 O10 C17 125.2(3) . . ? C11 O11 C18 122.9(2) . . ? C21 O20 C27 122.4(2) . . ? C25 O21 C28 118.7(3) . . ? C5 C1 C2 118.5(3) . . ? C5 C1 Ge1A 100.0(4) . . ? C2 C1 Ge1A 133.0(3) . . ? C5 C1 Ge1 125.8(3) . . ? C2 C1 Ge1 115.7(2) . . ? Ge1A C1 Ge1 36.2(2) . . ? O2 C2 C3 122.8(4) . . ? O2 C2 C1 115.9(3) . . ? C3 C2 C1 121.2(3) . . ? C4 C3 C2 118.9(4) . . ? C3 C4 C6 121.6(3) . . ? C4 C6 C5 119.9(4) . . ? O1 C5 C1 115.6(3) . . ? O1 C5 C6 124.3(3) . . ? C1 C5 C6 120.1(4) . . ? O1 C7 C7B 103.3(3) . . ? O1 C7 C7C 110.1(3) . . ? C7B C7 C7C 109.4(4) . . ? O1 C7 C7A 110.8(3) . . ? C7B C7 C7A 108.8(3) . . ? C7C C7 C7A 113.9(3) . . ? O2 C8 C8C 103.1(3) . . ? O2 C8 C8A 111.0(3) . . ? C8C C8 C8A 110.7(3) . . ? O2 C8 C8B 110.5(3) . . ? C8C C8 C8B 109.3(3) . . ? C8A C8 C8B 112.0(4) . . ? C11 C10 C15 117.6(3) . . ? C11 C10 Ge1 118.1(2) . . ? C15 C10 Ge1 123.6(2) . . ? C11 C10 Ge1A 140.1(3) . . ? C15 C10 Ge1A 99.5(3) . . ? Ge1 C10 Ge1A 32.8(2) . . ? C12 C11 O11 121.8(3) . . ? C12 C11 C10 122.0(3) . . ? O11 C11 C10 116.0(3) . . ? C13 C12 C11 118.6(3) . . ? C14 C13 C12 121.1(3) . . ? C13 C14 C15 119.9(3) . . ? O10 C15 C14 125.7(3) . . ? O10 C15 C10 113.6(3) . . ? C14 C15 C10 120.6(3) . . ? O10 C17 C17A 110.6(3) . . ? O10 C17 C17C 101.5(3) . . ? C17A C17 C17C 110.4(4) . . ? O10 C17 C17B 109.9(3) . . ? C17A C17 C17B 113.8(4) . . ? C17C C17 C17B 109.9(4) . . ? O11 C18 C18A 109.9(3) . . ? O11 C18 C18C 111.7(3) . . ? C18A C18 C18C 111.5(3) . . ? O11 C18 C18B 102.2(3) . . ? C18A C18 C18B 111.0(3) . . ? C18C C18 C18B 110.3(3) . . ? C25 C20 C21 117.5(3) . . ? C25 C20 Ge1 125.7(2) . . ? C21 C20 Ge1 116.3(2) . . ? C25 C20 Ge1A 104.7(3) . . ? C21 C20 Ge1A 132.0(3) . . ? Ge1 C20 Ge1A 35.6(2) . . ? C22 C21 O20 122.9(3) . . ? C22 C21 C20 121.6(3) . . ? O20 C21 C20 115.2(3) . . ? C21 C22 C23 119.5(3) . . ? C24 C23 C22 120.6(4) . . ? C23 C24 C25 119.6(3) . . ? C24 C25 O21 119.7(3) . . ? C24 C25 C20 121.1(3) . . ? O21 C25 C20 118.7(3) . . ? O20 C27 C27C 111.8(3) . . ? O20 C27 C27B 101.8(3) . . ? C27C C27 C27B 111.4(3) . . ? O20 C27 C27A 110.2(3) . . ? C27C C27 C27A 111.1(3) . . ? C27B C27 C27A 110.2(3) . . ? O21 C28 C28A 111.8(3) . . ? O21 C28 C28B 101.8(3) . . ? C28A C28 C28B 110.4(3) . . ? O21 C28 C28C 108.7(3) . . ? C28A C28 C28C 112.5(4) . . ? C28B C28 C28C 111.2(3) . . ? _diffrn_measured_fraction_theta_max 0.898 _diffrn_reflns_theta_full 26.05 _diffrn_measured_fraction_theta_full 0.898 _refine_diff_density_max 0.487 _refine_diff_density_min -0.674 _refine_diff_density_rms 0.063